Analysis Methods For N-butyl Amine And Other Ingredients In ZHP Zeolite Mother Liquor

In the production process of zeolite will produce a large of waste,which there are a large number of raw materials not being used,mainly containing template,sodium,a small amount of aluminum silicate ions and partial ion.If the molecular sieve liquor treated as liquid waste directly,the behavior not only wasted a lot of resources,but also polluted the environment.In order to comply with the background of green chemistry,the subject is for the determination of inorganic elements such as sodium,silicon and aluminum,and template n-butyl amine in ZHP zeolite liquor produced by Hunan Jianchang Petrochemical Co.Ltd.In order to recycle the zeolite mother liquor efficiently by the production company,the research is aim at developing methods for quantitative analysis.Around the main topic,the following four aspects had been studied:(1)Using the principle of gas chromatography,found a suitable capillary column and a suitable internal standard iso-propanol,which physical properties,chemical properties and GC retention time is similar to n-butyl amine,and does not react with n-butyl amine.The best conditions for gas chromatography had been explored.A rapid and feasible direct injection gas chromatography internal standard method to determent n-butyl amine in zeolite mother liquor had been established.Considering the high volatility of n-butyl amine,iso-octanol as the extractant had been selected to extract n-butyl amine in liquor,and then organic phase was used for gas chromatographic analysis.(2)Using principle of liquid chromatography,o-nitrobenzaldehyde had been chosen as the suitable derivative agent with a UV-absorbing group,which can fully react with n-butyl amine.The reaction conditions of amine-aldehyde condensation had been optimized.A performance liquid chromatography with pre-column derivation method for analysis of N-butyl amine in mother liquor of zeolite has been studied.The relative recoveries were 73.88%-99.68%,the RSD was less than 1%.This method is feasible for analyzing the concentrations of N-butyl amine in mother liquor of zeolite.(3)The phenomenon of gradient distribution of n-butyl amine in water tank in industrial process of zeolite synthesis had been found.To explore the reason for the phenomenon,a related simulation test had been carried out.A theoretical inference had been made from some meaningful results which been get from the simulation test.We can speculate about the reason for concentration gradient distribution is unrelated to natural evaporation of n-butyl amine.The reason may be due to the process of pouring the hot mother liquor in which the n-butyl amine could be carried to the upper layer by steam.The process may result in the upper level significantly higher than the lower level.(4)The content of sodium in the mother liquor had been determined by atomic absorption spectrometry.The content of silicon in the mother liquor had been determined by gravimetric method and volumetric method.The content of aluminum in the mother liquor had been determined by back titration and UV spectrophotometer.The precision and accuracy of all methods are satisfactory agreement with the requirement of detection.